Preparation method of fluoride-free single-crystal TiO2 nanometer thin film

A nano-thin film and single crystal technology, applied in the direction of single crystal growth, single crystal growth, chemical instruments and methods, etc., can solve the problems of passivating surface activity, reducing photocatalytic performance and photoelectric conversion performance, and achieve high controllability , high photocatalytic performance and photoelectric conversion performance, and wide application prospects

Inactive Publication Date: 2013-09-25
UNIV OF ELECTRONICS SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

(001) surface TiO prepared by traditional hydrothermal method 2 The surface of nanopowder contains a large number of fluorine ions, which seriously passivates the surface activity and reduces its photocatalytic performance and photoelectric conversion performance.

Method used

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  • Preparation method of fluoride-free single-crystal TiO2 nanometer thin film
  • Preparation method of fluoride-free single-crystal TiO2 nanometer thin film
  • Preparation method of fluoride-free single-crystal TiO2 nanometer thin film

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Experimental program
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Effect test

Embodiment 1

[0021] 1) Amorphous TiO was obtained by anodizing metal titanium sheets in fluorine-containing organic electrolyte (294 ml ethylene glycol, 6 ml water and 1 g ammonium fluoride). 2 Nanotube array films as precursors. It looks like figure 1 As shown, the length of the nanotube array can be controlled by adjusting parameters such as voltage and oxidation time;

[0022] 2) The obtained amorphous TiO 2 The nanotube array film precursor is soaked in an aqueous ammonium fluoride solution with a concentration of 0.1% by mass for 5 minutes, and taken out to dry for later use;

[0023] 3) The TiO treated in step 2) 2 The nanotube array film was placed in a closed container and calcined at 450 °C for 2 hours to obtain a single crystal anatase type (001) exposed TiO with fluorine on the surface 2 nano film. The SEM morphology of the film is shown in figure 2 As shown, the single-crystal anatase (001) exposed TiO contained 2 The particle size distribution of nanoparticles can be c...

Embodiment 2

[0026] 1) Using the method of anodizing metal titanium sheets, in the fluorine-containing organic electrolyte, obtain amorphous TiO 2 Nanotube array films as precursors;

[0027] 2) The obtained amorphous TiO 2 The nanotube array film precursor is soaked in an aqueous ammonium fluoride solution with a mass percent concentration of 0.5% for 5 minutes, and taken out to dry for later use;

[0028] 3) The TiO treated in step 2) 2 The nanotube array film is placed in a closed container and calcined at 500 ° C for 2 hours to obtain a single-crystal anatase (001) surface-exposed TiO with fluorine on the surface 2 nano film;

[0029] 4) TiO exposed on the fluorine-containing single crystal anatase (001) surface obtained in step 3) 2 Nano-film, further calcined in air at 500 ° C for 3 hours for defluorination treatment, that is, TiO with fluorine-free single crystal anatase (001) surface exposed 2 nano film.

Embodiment 3

[0031] 1) Using the method of anodizing metal titanium sheets, in the fluorine-containing organic electrolyte, obtain amorphous TiO 2 Nanotube array films as precursors;

[0032] 2) The obtained amorphous TiO 2 The nanotube array film precursor is soaked in an aqueous ammonium fluoride solution with a mass percent concentration of 1.0% for 4 minutes, and taken out to dry for later use;

[0033] 3) The TiO treated in step 2) 2The nanotube array film is placed in a closed container and calcined at 550 ° C for 1 hour to obtain a single-crystal anatase (001) surface-exposed TiO with fluorine on the surface 2 nano film;

[0034] 4) TiO exposed on the fluorine-containing single crystal anatase (001) surface obtained in step 3) 2 Nano-film, further calcined in air at 550 ° C for 2 hours for defluorination treatment, that is, TiO with fluorine-free single crystal anatase (001) surface exposed 2 nano film.

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Abstract

The invention provides a preparation method of a fluoride-free single-crystal TiO2 nanometer thin film and belongs to the technical field of functional materials. The preparation method using an amorphous state TiO2 nanotube array thin film as a precursor comprises the following steps of: firstly soaking the precursor in an ammonium fluoride aqueous solution so as to initialize the concentration of fluoride ions contained in the precursor; then calcining the precursor in a sealing container, so that the precursor collapses under the catalytic effect of the fluoride ions and the high-temperature effect and is converted into TiO nanometer particles the surfaces of which contain fluorine with exposed (001); finally, carrying out defluorination treatment at a high temperature to obtain the fluorine-free single-crystal TiO2 nanometer thin film. The TiO2 nanometer thin film prepared by the method has higher photocatalytic performance and photovoltaic conversion performance as well as wide application prospect in terms of solar photovoltaic devices, photolysis water, photocatalysis and the like. The preparation method adopts a two-step or multi-step later-period thermal treatment combination technology and has the advantages of high controllability, good repeatability, high production cost, low synthetic cost, large-scale manufacturing, and the like.

Description

technical field [0001] The invention belongs to the technical field of functional materials and relates to TiO 2 Nanofilms, especially defluorinated single-crystal anatase (001) exposed TiO 2 Preparation method of nanoparticle film. technical background [0002] TiO 2 It is a wide bandgap semiconductor with high catalytic activity, stable physical and chemical properties, and low cost. In recent years, high surface energy and high activity (001) surface TiO 2 The preparation and application of nanoparticles have attracted extensive attention from the scientific and engineering communities. While single crystal TiO 2 nanomaterials than polycrystalline TiO 2 Nanomaterials have more advantages and characteristics in the application of ordered heterojunctions, especially TiO with (001) surface exposure 2 Single-crystal nanoparticles exhibit higher photocatalytic and electrochemical activities. At present, various powdery (001) surface exposed TiO has been prepared by hyd...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/16C30B1/02
Inventor 廖宇龙张怀武钟智勇白飞明李颉
Owner UNIV OF ELECTRONICS SCI & TECH OF CHINA
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